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Benzoic Acid → N-(2-Aminoethyl)benzamide--hydrogen chloride (1/1)

HRID 2255106
ノート
印刷プレビュー

反応式

HRID 2255106 の反応式
[C:1]([OH:9])(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.[Cl:17]C(OCC)=O.[CH2:23]([NH2:26])[CH2:24][NH2:25]>C(Cl)(Cl)Cl>[ClH:17].[NH2:25][CH2:24][CH2:23][NH:26][C:1](=[O:9])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 243Benzoic AcidHCID 3301EthylenediamineHCID 8471TriethylamineHCID 10928Ethyl chloroformate

生成物 1

HCID 12715873N-(2-Aminoethyl)benzamide--hydrogen chloride (1/1)

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

24.4 g (0.02 mol) of benzoic acid are reacted with triethylamine and ethyl chloroformate in a manner analogous to that described in Example 5 and added dropwise at 10° to a solution of 53.5 ml (0.8 mol) of ethylenediamine in 750 ml of chloroform. After removing the difficulty soluble neutral constituents by filtration, the chloroform solution is concentrated and excess ethylenediamine is removed in a high vacuum. The oily residue (36.3 g) is taken up in 200 ml of 2N sodium hydroxide solution, saturated with solid sodium chloride and extracted several times with ethyl acetate. The ethyl acetate extracts are dried over magnesium sulfate and concentrated. The product is converted into the hydrochloride which is purified by recrystallization from ethanol, there being obtained 5.2 g of N-(2- aminoethyl)benzamide hydrochloride [J. Amer. Chem. Soc. 61, 822 (1939)], m.p. 163°-165°.

後処理

  1. customAfter removing the difficulty soluble neutral constituents
  2. filtrationby filtration
  3. concentrationthe chloroform solution is concentrated
  4. customexcess ethylenediamine is removed in a high vacuum
  5. extractionextracted several times with ethyl acetate
  6. dry with materialThe ethyl acetate extracts are dried over magnesium sulfate
  7. concentrationconcentrated
  8. customis purified by recrystallization from ethanol, there

出典と根拠

ORDレコード
ord-08ee53e67ff54b3a854e411a11cf780b
出典データセット
uspto-grants-1993_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05238962

反応ノート

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